反应详情

1.5 g (3.95 mmol) of 2-chloro-6-(3-cyano-phenyl-amino)-purine, 2.1 g (6.3 mmol) of caesium carbonate and 2.6 ml (31.6 mmol) of iodoethane are stirred in 66 ml of a mixture comprising dioxane:water:DMF in a ratio of 1:2:3 at RT for 19 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water. After drying over sodium sulfate, the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1). After removal of the solvent, 2-chloro-9-ethyl-6-(3-cyano-phenyl-amino)-9H-purine is obtained as a crystalline precipitate. This precipitate is filtered off and dried; m.p. 189° C.; FAB-MS: (M+H)+=299; Rf=0.9 (CH2Cl2:methanol 9:1).

1. washthe organic phase is washed with water
2. dry with materialAfter drying over sodium sulfate
3. customthe residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1)
4. customAfter removal of the solvent